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    有机相进样-电感耦合等离子体原子发射光谱法测定植物油脂中聚二甲基硅氧烷的含量

    Determination of Polydimethylsiloxane in Vegetable Oil by Organic Phase Sampling-Inductively Coupled Plasma Atomic Emission Spectrometry

    • 摘要: 为解决现有测定植物油脂中聚二甲基硅氧烷的电感耦合等离子体原子发射光谱法(ICP-AES)存在因标准溶液与样品基质差异较大、塑料材质溶出硅而导致测定结果偏高的问题,提出了题示方法,并考察了稀释剂的类型和性质、稀释比例以及容器材质对测定结果的影响。试验得出有利于等离子体稳定的稀释剂参数范围:蒸气压(20 ℃) 0.032~0.287 kPa,密度(20 ℃) 0.798~0.881 g·mL-1,运动黏度(20 ℃) 2.47~15.8 mm2·s-1。当待测溶液的运动黏度(20 ℃)小于6.35 mm2·s-1时,工作曲线的相关系数大于0.999 5,以ICP溶剂为稀释剂,当植物油脂与稀释剂的稀释比例为1∶4(质量比)时,方法检出限较低。在聚二甲基硅氧烷的提取过程中,不论塑料离心管是否经过加热处理均会使提取液中的待测物质含量有着不同程度的增加,玻璃材质的比色管则无影响。优化的试验条件如下:取4 g样品置于50 mL玻璃比色管中,加入ICP溶剂至总质量为20 g,混匀,于70 ℃超声提取2 h,再加入15 mL 1.37 mol·L-1盐酸溶液充分混匀,静置分层,取上清液置于玻璃比色管中,采用ICP-AES测定其中聚二甲基硅氧烷的含量。结果表明,通过加入适量的空白植物油脂的基质匹配法有效校正了样品基质对测定结果的干扰,聚二甲基硅氧烷的质量分数在0.500~10.0 mg·kg-1内与对应的硅元素发射强度呈线性关系,检出限为0.30 mg·kg-1。按照标准加入法进行回收试验,回收率为95.6%~106%,测定值的相对标准偏差(n=7)为1.1%~3.4%。采用本法与GB 5009.254-2016第二法火焰原子吸收光谱法测定同一实际加标样品,两种方法所得测定结果一致。

       

      Abstract: In order to solve the problem of high determination results caused by significant differences between the standard solution and the sample matrix, and the dissolution of silicon from plastic materials in the existing method of inductively coupled plasma atomic emission spectrometry (ICP-AES) for the determination of polydimethylsiloxane in vegetable oil, the method mentioned by title was proposed, and effects of the types and properties of diluents, dilution ratios, and container materials on the determination results were investigated. The range of diluent parameters which was beneficial for plasma stabilization was optimized by the test, with vapor pressure (20 ℃) from 0.032 kPa to 0.287 kPa, density (20 ℃) from 0.798 g·mL-1 to 0.881 g·mL-1, and kinematic viscosity (20 ℃) from 2.47 mm2·s-1 to 15.8 mm2·s-1. When the kinematic viscosity (20 ℃) of the solution to be tested was less than 6.35 mm2·s-1, the correlation coefficient of the working curve was above 0.999 5. When the dilution ratio of vegetable oil to diluent was 1∶4 (mass ratio), the detection limit of the method was lower, using ICP solvent as the diluent. In the extraction process of polydimethylsiloxane, no matter whether the plastic centrifuge tube was heated or not, the content of the substance to be tested in the extraction solution increased to varying degrees, while there was no effect using the colorimetric tube made of glass material. The optimized experimental conditions were as follows. The sample (4 g) was taken and placed in a 50 mL-glass colorimetric tube. ICP solvent was added till to a total mass of 20 g, and then the mixture was mixed well and extracted by ultrasonic for 2 h at 70 ℃. 15 mL of 1.37 mol·L-1 hydrochloric acid solution was added, following mixing well and settling to layer. The supernatant was taken and placed into a glass colorimetric tube, in which polydimethylsiloxane was determined by ICP-AES. As shown by the results, the matrix matching method effectively corrected the interference of the sample matrix on the determination results by adding an appropriate amount of blank vegetable oil. Linear relationship between values of the corresponding emission intensity of silicon element and mass fraction of polydimethylsiloxane was found in the range of 0.500-10.0 mg·kg-1, with lower limit of determination of 0.30 mg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 95.6%-106%, with RSDs (n=7) of the determined values in the range of 1.1%-3.4%. This method and flame atomic absorption spectrometry of GB 5009.254-2016 second method were applied to determination of the same actual spiked sample, and the determination results obtained by two methods were consistent.

       

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